Synthesis and crystal structure of the cubane-like cluster [(Tp*)MoFe₃S₃(μ₃-Cl)(PMe₃)₃](BPh₄)

The title compound, μ₃-chlorido-tri-μ₃-sulfido-tris-(tri-methyl-phosphine)[tris-(3,5-di-methyl-pyrazol-1-yl)hydro-borato]triiron(II)molybdenum(III) tetra-phenyl-borate, [MoFe₃S₃Cl(C₁₅H₂₂BN₆)(C₉H₂₇P₃)](C₂₄H₂₀B) or [(Tp*)MoFe₃S₃(μ₃-Cl)(PMe₃)₃](BPh₄) [Tp* = tris-(3,5-di-methyl-pyrazol-1-yl)hydro- borate(1-)], crystallizes as block-shaped crystals in space group P1. In this cluster, the Mo site is in a distorted octa-hedral coordination model, coordinating to three N atoms on the Tp* ligand and three μ₃-bridging S atoms in the core. The Fe sites adopt a distorted tetra-hedral coordination geometry, each coordinating to two μ₃-bridging S atoms, one μ₃-bridging Cl atom, and the phospho-rus atom from a tri-methyl-phosphine ligand. This type of heterometallic and heteroleptic single cubane cluster represents a typical example within the Mo-Fe-S cluster family. It may possess unique advantages in the construction of high-nuclearity clusters, and could serve as a potentially controllable reaction inter-mediate for the synthesis of FeMo-co mimics. The residual electron density of disordered solvent mol-ecules in the void space could not be reasonably modeled, thus a solvent mask was applied. The solvent contribution is not included in the reported mol-ecular weight and density.